CN111848390A - Method for treating itaconic acid mother liquor and recovering itaconic acid - Google Patents
Method for treating itaconic acid mother liquor and recovering itaconic acid Download PDFInfo
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- CN111848390A CN111848390A CN202010755436.7A CN202010755436A CN111848390A CN 111848390 A CN111848390 A CN 111848390A CN 202010755436 A CN202010755436 A CN 202010755436A CN 111848390 A CN111848390 A CN 111848390A
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- itaconic acid
- tower
- mother liquor
- extraction
- treating
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- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 title claims abstract description 76
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000012452 mother liquor Substances 0.000 title claims abstract description 35
- 238000000605 extraction Methods 0.000 claims abstract description 47
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000000855 fermentation Methods 0.000 description 13
- 230000004151 fermentation Effects 0.000 description 13
- 239000002699 waste material Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002921 fermentation waste Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/445—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by steam distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for treating itaconic acid mother liquor to recover itaconic acid and a device suitable for the method. According to the method, ethyl acetate is used as an extracting agent, itaconic acid mother liquor and the extracting agent ethyl acetate enter an extracting tower for extraction and separation, extract liquid enters a stripping tower for separation, the extracting agent is obtained by recycling the top of the stripping tower through a condenser, itaconic acid and water at the bottom of the extracting tower are obtained by passing through a crystallizer and a separator, and a water phase is recycled to the extracting tower. The method has the advantages of low energy consumption, simple process, high extraction efficiency, and economic and easy recovery of the adopted extractant ethyl acetate.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of chemical separation and purification, particularly relates to a method for treating itaconic acid mother liquor and recovering itaconic acid, and further relates to a method for separating itaconic acid from itaconic acid mother liquor by extraction, distillation and crystallization methods by taking an organic solvent as an extracting agent.
[ background of the invention ]
The prior industrial production methods of itaconic acid comprise a chemical synthesis method and a fermentation method. Compared with the chemical synthesis method, the fermentation method has more advantages, and most of itaconic acid is produced internationally by the fermentation method, but the fermentation method has the defects of simple process equipment, less investment, fast operation, simple operation technology, low energy consumption, extensive raw materials and the like, and itaconic acid in the fermentation liquid is difficult to extract. At present, the method for separating and extracting itaconic acid from fermentation liquor is a recrystallization method, but a large amount of waste liquor is generated in the separation process, so that on one hand, the loss of enterprises is great, and on the other hand, the environmental protection treatment is difficult due to the mother liquor with the CODcr as high as 60-80 ten thousand mg/L.
The itaconic acid fermentation waste liquid is fermentation industrial waste water which is extremely difficult to treat and has the advantages of suspended matters, more solid matters, large viscosity, low pH value and deep chroma, and an effective treatment method for the waste liquid is not available at present. In order to improve the recovery rate of the itaconic acid, a scheme for recovering the itaconic acid from the fermentation waste liquid by an extraction method is discussed.
Chinese patent CN201210303823.2 discloses a method for extracting itaconic acid from itaconic acid fermentation broth, wherein the extraction rate of itaconic acid is 89%.
Chinese patent 20071019534.5 discloses a method for extracting itaconic acid from itaconic acid fermentation broth or itaconic acid product mother liquor, which adopts high performance liquid chromatography to extract itaconic acid, but needs to prepare synthetic resin, and the process is complex.
The existing method for extracting itaconic acid from fermentation mother liquor has the problems of resource waste, low removal rate, complex process and the like.
The method combines extraction, distillation and crystallization to separate itaconic acid from itaconic acid mother liquor, takes ethyl acetate as an extracting agent, can save a large amount of acid and alkali loss, has short process flow in comparison, and is an ideal extraction method.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a device for treating itaconic acid mother liquor and recovering itaconic acid.
It is another object of the present invention to provide a process for treating a mother liquor of itaconic acid fermentation and recovering itaconic acid using said apparatus.
It is another object of the present invention to provide the use of an organic solvent as an extractant in the recovery of itaconic acid in a fermentation mother liquor.
[ solution ]
The invention is realized by the following technical scheme.
A method for treating itaconic acid mother liquor to recover itaconic acid is characterized in that a device for realizing the method mainly comprises the following parts: an extraction tower (T1), a stripping tower (T2), a crystallizer (M1), a condenser (C1), a centrifuge (L1) and a pump (P1); wherein the top of the extraction tower (T1) is connected with a stripping tower (T2), the top of the stripping tower (T2) is connected with a condenser (C1) to recover an extracting agent, the bottom of the stripping tower (T2) is sequentially connected with a crystallizer (M1) and a centrifuge (L1), and the water phase of the centrifuge (L1) is circulated back to the extraction tower (T1) through a pump (P1).
The method for treating the itaconic acid mother liquor and recycling the itaconic acid by adopting the device comprises the following steps:
(1) the itaconic acid mother liquor enters from the top of an extraction tower (T1), the extractant enters from the bottom of the extraction tower (T1), after effective contact extraction and separation, a raffinate phase and extractant mixture is discharged from the bottom of the extraction tower (T1), and an extract phase itaconic acid and extractant mixture enters a stripping tower (T2) from the top of the extraction tower (T1);
(2) after the itaconic acid mother liquor is separated by a stripping tower (T2), an extractant enters a condenser (C1) from the top to be recovered, water and itaconic acid enter a crystallizer (M1) from the bottom of the tower, the water and the itaconic acid enter a centrifuge (L1) to be centrifuged to separate the itaconic acid, and a water phase is recovered to an extraction tower (T1) to be recycled by a pump (P1).
The extraction agent is ethyl acetate, the operating pressure of the extraction tower (T1) is 1atm, the number of tower plates is 5-10, the pressure of the stripping tower (T2) is 1atm, the number of tower plates is 9-18, and the recovery rate of itaconic acid in the itaconic acid mother liquor is higher than 92.7%.
[ advantageous effects ]
Compared with the prior art, the invention mainly has the following beneficial effects:
(1) the method for extracting the itaconic acid can obtain the itaconic acid with good extraction effect, and solves the problem of difficult extraction of the itaconic acid from the fermentation mother liquor.
(2) The method has the advantages of simple process, less investment equipment, high extraction rate in the process and the like, and the adopted extractant, namely the ethyl acetate, is low in economic pollution.
(3) The extraction agent ethyl acetate adopted in the method is easy to recover, the loss of the extraction agent is reduced, and the separation cost is reduced.
[ description of the drawings ]
FIG. 1 is a flow diagram of a process for treating itaconic acid mother liquor to recover itaconic acid in accordance with the present invention.
In the figure, T1-extraction column; t2-stripper column; c1-condenser; m1-crystallizer; l1-separator; p1-pump; the extractant and itaconic acid mother liquor feeds are labeled in the figure.
[ detailed description ] embodiments
Example 1:
the feed flow is 1000kg/h, the feed is itaconic acid mother liquor, and the number of theoretical plates of the extraction column (T1) is 10. The itaconic acid mother liquor enters from the top of an extraction tower (T1), an extracting agent enters from the bottom of the extraction tower (T1), the extracting agent is ethyl acetate, the flow rate is 800kg/h (the mass ratio of the feeding flow rate of the extracting agent to the itaconic acid mother liquor is 0.8), and the temperature of the extraction tower (T1) is 26 ℃. The number of plates of the stripping tower (T2) is 9, the pressure is 1atm, a full condenser is adopted at the top of the tower, and a reboiler is not arranged at the bottom of the tower. The recovery of itaconic acid was 92.7%.
Example 2:
the feed flow is 1000kg/h, the feed is itaconic acid mother liquor, and the number of theoretical plates of the extraction column (T1) is 12. The itaconic acid mother liquor enters from the top of an extraction tower (T1), the extractant enters from the bottom of the extraction tower (T1), the extractant is ethyl acetate, the flow rate is 1500kg/h (the mass ratio of the feeding flow rate of the extractant to the itaconic acid mother liquor is 1.5), and the temperature of the extraction tower (T1) is 28 ℃. The number of plates of the stripping tower (T2) is 15, the pressure is 1atm, a full condenser is adopted at the top of the tower, and a reboiler is not arranged at the bottom of the tower. The recovery of itaconic acid was 93.2%.
Example 3:
the feed flow is 1000kg/h, the feed is itaconic acid mother liquor, and the number of theoretical plates of the extraction column (T1) is 15. The itaconic acid mother liquor enters from the top of an extraction tower (T1), an extracting agent enters from the bottom of the extraction tower (T1), the extracting agent is ethyl acetate, the flow rate is 2200kg/h (the mass ratio of the feeding flow rate of the extracting agent to the itaconic acid mother liquor is 2.2), and the temperature of the extraction tower (T1) is 29.7 ℃. The number of plates of the stripping tower (T2) is 18, the pressure is 1atm, a full condenser is adopted at the top of the tower, and a reboiler is not arranged at the bottom of the tower. The recovery of itaconic acid was 92.9%.
Claims (1)
1. A method for treating itaconic acid mother liquor to recover itaconic acid is characterized in that a device for realizing the method mainly comprises the following parts: an extraction tower (T1), a stripping tower (T2), a crystallizer (M1), a condenser (C1), a centrifuge (L1) and a pump (P1); wherein the top of the extraction tower (T1) is connected with a stripping tower (T2), the top of the stripping tower (T2) is connected with a condenser (C1) to recover an extracting agent, the bottom of the stripping tower (T2) is sequentially connected with a crystallizer (M1) and a centrifuge (L1), the water phase of the centrifuge (L1) is circulated back to the extraction tower (T1) through a pump (P1),
the method for treating the itaconic acid mother liquor and recycling the itaconic acid by adopting the device comprises the following steps:
(1) the itaconic acid mother liquor enters from the top of an extraction tower (T1), the extractant enters from the bottom of the extraction tower (T1), after effective contact extraction separation, a raffinate phase and extractant mixture is discharged from the bottom of the extraction tower (T1), an extract phase itaconic acid and extractant mixture enters into a stripping tower (T2) from the top of the extraction tower (T1),
(2) after the itaconic acid mother liquor is separated by a stripping tower (T2), an extractant enters a condenser (C1) from the top to be recovered, water and itaconic acid enter a crystallizer (M1) from the bottom of the tower, the water and the itaconic acid enter a centrifuge (L1) after being crystallized to separate the itaconic acid, a water phase is recovered to an extraction tower (T1) by a pump (P1) to be recycled,
the extraction agent is ethyl acetate, the operating pressure of the extraction tower (T1) is 1atm, the number of tower plates is 5-10, the pressure of the stripping tower (T2) is 1atm, the number of tower plates is 9-18, and the recovery rate of itaconic acid in the itaconic acid mother liquor is higher than 92.7%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010755436.7A CN111848390A (en) | 2020-07-31 | 2020-07-31 | Method for treating itaconic acid mother liquor and recovering itaconic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010755436.7A CN111848390A (en) | 2020-07-31 | 2020-07-31 | Method for treating itaconic acid mother liquor and recovering itaconic acid |
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| CN111848390A true CN111848390A (en) | 2020-10-30 |
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| CN202010755436.7A Pending CN111848390A (en) | 2020-07-31 | 2020-07-31 | Method for treating itaconic acid mother liquor and recovering itaconic acid |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085734A (en) * | 2007-06-25 | 2007-12-12 | 江南大学 | Method for purifying itaconic acid fermentation liquor or extracting itaconic acid from itaconic acid mother liquid by film device |
| CN101186571A (en) * | 2007-11-30 | 2008-05-28 | 江南大学 | Method for purifying itaconic acid from itaconic acid fermentation liquor or itaconic acid product mother liquid |
| US7479381B1 (en) * | 2006-12-15 | 2009-01-20 | The United States Of America As Represented By The Secretary Of Agriculture | Production of itaconic acid by Pseudozyma antarctica |
| CN101898952A (en) * | 2010-07-19 | 2010-12-01 | 天津市天大北洋化工设备有限公司 | Method and device for treating low-concentration acetic acid wastewater |
| CN102408325A (en) * | 2011-11-29 | 2012-04-11 | 青岛琅琊台集团股份有限公司 | Method for extracting itaconic acid from itaconic acid fermentation waste mother solution |
| CN102816056A (en) * | 2012-08-24 | 2012-12-12 | 青岛科海生物有限公司 | Method for extracting itaconic acid through extraction of itaconic acid fermentation solution |
| CN102816055A (en) * | 2012-08-24 | 2012-12-12 | 青岛琅琊台集团股份有限公司 | Novel process of treatment of waste mother solution for itaconic acid fermentation through seawater desalination and membrane separation |
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| CN105439845A (en) * | 2015-12-16 | 2016-03-30 | 浙江国光生化股份有限公司 | Method for extracting itaconic acid crystals from itaconic acid mother liquor |
-
2020
- 2020-07-31 CN CN202010755436.7A patent/CN111848390A/en active Pending
Patent Citations (9)
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|---|---|---|---|---|
| US7479381B1 (en) * | 2006-12-15 | 2009-01-20 | The United States Of America As Represented By The Secretary Of Agriculture | Production of itaconic acid by Pseudozyma antarctica |
| CN101085734A (en) * | 2007-06-25 | 2007-12-12 | 江南大学 | Method for purifying itaconic acid fermentation liquor or extracting itaconic acid from itaconic acid mother liquid by film device |
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| CN101898952A (en) * | 2010-07-19 | 2010-12-01 | 天津市天大北洋化工设备有限公司 | Method and device for treating low-concentration acetic acid wastewater |
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| CN102816056A (en) * | 2012-08-24 | 2012-12-12 | 青岛科海生物有限公司 | Method for extracting itaconic acid through extraction of itaconic acid fermentation solution |
| CN102816055A (en) * | 2012-08-24 | 2012-12-12 | 青岛琅琊台集团股份有限公司 | Novel process of treatment of waste mother solution for itaconic acid fermentation through seawater desalination and membrane separation |
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Application publication date: 20201030 |